N,N'-Bis(methyl 3,4,6-tri-O-acetyl-2-deoxy-b-D-glucopyranosid-2-yl)urea 1 and its N'-nitroso derivative 2 were synthesized from methyl 2-amino-3,4,6-tri-O-acetyl-2-deoxy-b-D-glucopyranoside and di(4-nitrophenyl)carbamate. The nitrosation was carried out using N2O3 in dichloromethane. The structure of compounds was analyzed by 1H, 13C, 15N NMR in CDCl3 and 13C CP MAS in the solid state. The assignments of resonances were done by COSY1H, 13C, HETCOR and the 1H, 15N2D correlation spectroscopy. Compound 1 gives one set of 1H/13C resonances in solution, but exhibits polymorphism in the solid state.
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